反应详情

23.4 G (0.1 mole) of 2,3,6-trichloroquinoxaline and 1 g of copper-I chloride (approximately 0.1 mole) were dissolved in 250 ml of anhydrous acetonitrile and 45 ml (approximately 2 moles) of liquid ammonia were added thereto. The reaction mixture was heated for 12 hours to 150°C in a steel autoclave of 0.7 liter capacity. In the course thereof, a pressure of 10 to 15 atmospheres gauge was set up. The crystalline precipitate produced after cooling was filtered off and dissolved in dilute sodium hydroxide solution. The solution was filtered, the filtrate was acidified with hydrochloric acid and the precipitate was filtered off, well rinsed with water and recrystallized from 30% strength acetic acid. 10 g (representing 46% of theory) of 6-chloro-2-methyl-1H-imidazo[4,5-b]quinoxaline of melting point >300°C were obtained.

1. customThe crystalline precipitate produced
2. temperatureafter cooling
3. filtrationwas filtered off
4. dissolutiondissolved in dilute sodium hydroxide solution
5. filtrationThe solution was filtered
6. filtrationthe precipitate was filtered off
7. washwell rinsed with water
8. customrecrystallized from 30% strength acetic acid